#------------------------------------------------------------------------------
#$Date: 2019-11-25 14:58:50 +0100 (lun 25 de nov de 2019) $
#$Revision: 241266 $
#$URL: svn://www.crystallography.net/cod/cif/4/13/09/4130914.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4130914
loop_
_publ_author_name
'Zhao, Xiang'
'Bu, Xianhui'
'Nguyen, Edward T.'
'Zhai, Quan-Guo'
'Mao, Chengyu'
'Feng, Pingyun'
_publ_section_title
;
 Multivariable Modular Design of Pore Space Partition.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15102
_journal_page_last               15105
_journal_paper_doi               10.1021/jacs.6b07901
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C30 H18 Fe4 Mg N9 O19'
_chemical_formula_sum            'C30 H18 Fe4 Mg N9 O19'
_chemical_formula_weight         1056.24
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.857(7)
_cell_length_b                   13.857(7)
_cell_length_c                   17.925(9)
_cell_measurement_reflns_used    225
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      19.27
_cell_measurement_theta_min      2.27
_cell_volume                     2981(3)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      174(2)
_diffrn_measured_fraction_theta_full 0.728
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART Apex diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2279
_diffrn_reflns_av_unetI/netI     0.1725
_diffrn_reflns_Laue_measured_fraction_full 0.728
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6078
_diffrn_reflns_point_group_measured_fraction_full 0.728
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.445
_diffrn_reflns_theta_min         1.697
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/3
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         772
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1848
_refine_ls_R_factor_gt           0.1072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1682P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2730
_refine_ls_wR_factor_ref         0.3160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                401
_reflns_number_total             772
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b07901_si_002.cif
_cod_data_source_block           CPM-420
_cod_database_code               4130914
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.74670(17) 0.4934(3) 0.2500 0.0381(14) Uani 1 4 d S T P
Fe2 Fe 1.0000 1.0000 0.3552(4) 0.056(3) Uani 0.47(3) 6 d S T P
Mg2 Mg 1.0000 1.0000 0.3552(4) 0.056(3) Uani 0.53(3) 6 d S T P
O2 O 0.6497(7) 0.5059(7) 0.3324(4) 0.033(2) Uani 1 1 d . . .
O1 O 0.6667 0.3333 0.2500 0.005(5) Uani 1 12 d S TU P
C2 C 0.5289(7) 0.4711(7) 0.4331(8) 0.023(4) Uani 1 2 d S T P
C3 C 0.5987(10) 0.5698(10) 0.4660(7) 0.042(4) Uani 1 1 d . . .
H3 H 0.6661 0.6188 0.4433 0.050 Uiso 1 1 calc R U .
C1 C 0.5616(6) 0.4384(6) 0.3591(9) 0.027(4) Uani 1 2 d S TU P
O3 O 1.0835(11) 1.167(2) 0.4314(13) 0.160(10) Uani 1 2 d S TU P
N1 N 0.8370(10) 0.6741(19) 0.2500 0.050(6) Uani 1 4 d DS TU P
N2 N 0.9273(9) 0.8546(17) 0.2910(8) 0.086(6) Uani 1 2 d DS TU P
C4 C 0.8706(9) 0.7412(19) 0.3061(12) 0.075(6) Uani 1 2 d DS TU P
H4 H 0.8573 0.7147 0.3549 0.090 Uiso 1 2 calc R U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Fe1 O2 94.2(3) . 16_556
O1 Fe1 O2 94.2(3) . 20_655
O2 Fe1 O2 171.7(5) 16_556 20_655
O1 Fe1 O2 94.2(3) . 11_655
O2 Fe1 O2 87.9(5) 16_556 11_655
O2 Fe1 O2 91.5(5) 20_655 11_655
O1 Fe1 O2 94.2(3) . .
O2 Fe1 O2 91.5(5) 16_556 .
O2 Fe1 O2 87.9(5) 20_655 .
O2 Fe1 O2 171.7(5) 11_655 .
O1 Fe1 N1 180.0 . .
O2 Fe1 N1 85.8(3) 16_556 .
O2 Fe1 N1 85.8(3) 20_655 .
O2 Fe1 N1 85.8(3) 11_655 .
O2 Fe1 N1 85.8(3) . .
N2 Fe2 N2 92.6(7) 2_765 .
N2 Fe2 N2 92.6(7) 2_765 3_675
N2 Fe2 N2 92.6(7) . 3_675
C1 O2 Fe1 132.0(9) . .
Fe1 O1 Fe1 120.0 . 3_665
Fe1 O1 Fe1 120.0 . 2_655
Fe1 O1 Fe1 120.000(1) 3_665 2_655
C3 C2 C3 119.3(15) . 19_665
C3 C2 C1 120.4(8) . .
C3 C2 C1 120.4(8) 19_665 .
C2 C3 C3 120.4(8) . 7_556
O2 C1 O2 126.9(16) . 19_665
O2 C1 C2 116.5(8) . .
O2 C1 C2 116.5(8) 19_665 .
C4 N1 C4 103(3) . 16_556
C4 N1 Fe1 128.7(14) . .
C4 N1 Fe1 128.7(14) 16_556 .
C4 N2 N2 101.3(10) . 16_556
C4 N2 Fe2 135.3(12) . .
N2 N2 Fe2 123.4(5) 16_556 .
N1 C4 N2 117(2) . .
N1 C4 C4 38.7(14) . 16_556
N2 C4 C4 78.7(10) . 16_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 1.921(4) .
Fe1 O2 2.061(8) 16_556
Fe1 O2 2.061(8) 20_655
Fe1 O2 2.061(8) 11_655
Fe1 O2 2.061(8) .
Fe1 N1 2.17(2) .
Fe2 N2 2.090(19) 2_765
Fe2 N2 2.090(19) .
Fe2 N2 2.090(19) 3_675
O2 C1 1.205(10) .
O1 Fe1 1.921(4) 3_665
O1 Fe1 1.921(4) 2_655
C2 C3 1.353(13) .
C2 C3 1.353(13) 19_665
C2 C1 1.54(2) .
C3 C3 1.40(2) 7_556
C1 O2 1.205(10) 19_665
N1 C4 1.29(2) .
N1 C4 1.29(2) 16_556
N2 C4 1.39(2) .
N2 N2 1.47(3) 16_556
C4 C4 2.01(4) 16_556
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.333 0.667 0.250 573 148 ' '
2 0.667 0.333 0.750 573 148 ' '
